Greenish-black sulfur dye and method of making same.



' UNITE STATES PATENT OF ICE.

ANTON PFENNIGER, on BRUGG, SWITZERLAND, ASSIGNQR TO THE FIRM OF OIIEMISCHE FABRIK BRUGG A. e, VORMALS DR. ZIMMERMANN & 00., OF

BRUGG, SWITZERLAND.

GREENlSH-BLACK SULFUR DYE AND METHOD OF MAKING SAME.

SPECIFICATION forming part of Letters Patent N 0. 698,220, dated April 22, 1902.

Application filed $eptember 6,1901. Serial No; 74,556. (No specimens.)

$ a. whom it may concern:

Be it known that I, ANTON PFENNIGER,3. citizen of the Swiss Republic, residing at Brugg, canton of Argovie, Switzerland, have invented new and useful Improvements in the Manufacture of Greenish-Black Directly-Dyeing Sulfurized Dyestufis for Cotton, of which the 'followingisaclear and complete specification.

The invention relates to the manufacture 1c of new greenish-black directly-dyeing sulfurized dyestuffs for cotton bysulfu rizing a paratoluene sulfonate.

The following example illustrates the invention: Into one hundred kilos of fused crystallized sodium sulfid are introduced twenty-one kilos of sodium paratoluene sulfonate, and the mixture is heated for about one hour While stirring at a temperature of 130 to 150 centigrade. After adding sixteen kilos of powdered sulfur the mixture is then heated at from 280 to 300 centigradeand kept at this temperature, while still stirring, until the formation of yellow vapors has ceased and a sample removed from the mass dissolves in 2 5 water to a dark greenish-black solution. The mass is then allowed to cool, when it may be used directly in dyeing. It dissolves in water to a greenish-black solution, from which the dyestuff may be precipitated in the form of brown flocks by adding acid. These flocks are insoluble in pure water and in water containing sodium carbonate; but they dissolve in caustic-soda solution and in aqueous solutions of sodium sulfid.'.

The dyestuff dyes in hot baths containing sodium sulfid, sodium carbonate, and com mon salt or sodium -sulfid,sodium carbonate, and sodium sulfate. The shades are greenish black and are very fast to light.

For sulfur and an alkali sulfid may be substituted alkali polysulfids or sulfur and an 7 alkali.

The proportion of the sulfurizing agent used, as well as the duration of the heating, can be varied.

' What I claim is- 1. The described process for the m anufac-v ture of greenish-black, sulfurized, directly dyeing dyestuffs for cotton, by heating a paratoluene sulfonate with sulfurizing agents.

2. As a new article of manufacture, the described greenish-black, sulfurized dyestufl, derived from a paratoluene sulfonate, which dyes unmordanted cotton, in a bath containing alkali sulfid, sodium carbonate and com mon salt, in greenish black shades fast to light.

my name, this 23d day of August, 1901, in

the presence of two subscribing witnesses.

ANTON PFENNIGER.

Witnesses:

WILLY HOMBERGER, J OSEPH VOLTZ.

In witness whereof I have hereunto signed 

